CAJ | 학술논문

目的介绍修订后的尿碘测定标准方法,即尿中碘的过硫酸铵消化-低砷量砷铈催化分光光度测定方法.方法修订后的新方法包括:改进的0.0～300.0μg/L范围尿碘测定步骤、新增加的300.0～1200.0μg/L范围尿碘测定步骤,每份尿碘检测所用的亚砷酸试剂量仅为现行标准法的1/4.对修订后的新方法进行评价,计算标准曲线线性关系及线性范围、样品测定检测限、精密度、准确度.结果尿碘含量为0.0～300.0μg/L、300.0～1200.0 μg/L的标准曲线按碘质量浓度(C)与测定吸光度(A)的定量关系为(C=a+b×lg/A),线性相关系数范围分别为-0.9995～-1.0000、-0.9994～-1.0000;尿碘检出限为2.0 μg/L(取样量为0.25 ml)；精密度:对尿碘35.6～265.5 μg/L的12个尿样各重复测定6次,相对标准偏差(RSD)范围为0.9％ (0.6/70.3)～3.3％(1.2/35.6),平均为1.8％；对尿碘330,0～1112.0μg/L的12个尿样各重复测定6次,RSD范围为0.4％(2.0/517.3)～2.2％ (7.2/330.1),平均为1.2％.准确度:对尿碘33.7～203.0μg/L的15个尿样加碘标回收率范围为93.8％(93.8/100)～103.9％(103.9/100),平均为99.4％;对含碘330.0 ～ 783.0μg/L的15个尿样加碘标回收率范围为91.2％(501.8/550)～102.9％(411.7/400),平均为98.2％；分别在不同反应温度下测定尿碘73.0、88.0、175.0、206.0、212.0 μg/L的5种尿碘标准物,相对误差范围为-2.8％(-5.9/212)～3.9％(6.9/175)；测定尿碘556.0μg/L和883.0μg/L的2种高尿碘标准物,相对误差范围为-0.7％(-7.0/883)～1.5％(8.1/556),测定结果均在给定值的不确定度范围内.结论修订后的新方法比原标准方法大幅减少了废液含砷量,减少了环境污染并节省了试剂.可直接取高碘尿样进行消化测定,避免了原标准方法测定高碘尿样需多倍稀释的稀释误差和操作不便,简便易操作,并提高了测定精密度和准确度.
목적 개소수정후적뇨전측정표준방법,즉뇨중전적과류산안소화-저신량신시최화분광광도측정방법.방법 수정후적신방법포괄:개진적0.0～300.0μg/L범위뇨전측정보취、신증가적300.0～1200.0μg/L범위뇨전측정보취,매빈뇨전검측소용적아신산시제량부위현행표준법적1/4.대수정후적신방법진행평개,계산표준곡선선성관계급선성범위、양품측정검측한、정밀도、준학도.결과 뇨전함량위0.0～300.0μg/L、300.0～1200.0 μg/L적표준곡선안전질량농도(C)여측정흡광도(A)적정량관계위(C=a+b×lg/A),선성상관계수범위분별위-0.9995～-1.0000、-0.9994～-1.0000;뇨전검출한위2.0 μg/L(취양량위0.25 ml)；정밀도:대뇨전35.6～265.5 μg/L적12개뇨양각중복측정6차,상대표준편차(RSD)범위위0.9％ (0.6/70.3)～3.3％(1.2/35.6),평균위1.8％；대뇨전330,0～1112.0μg/L적12개뇨양각중복측정6차,RSD범위위0.4％(2.0/517.3)～2.2％ (7.2/330.1),평균위1.2％.준학도:대뇨전33.7～203.0μg/L적15개뇨양가전표회수솔범위위93.8％(93.8/100)～103.9％(103.9/100),평균위99.4％;대함전330.0 ～ 783.0μg/L적15개뇨양가전표회수솔범위위91.2％(501.8/550)～102.9％(411.7/400),평균위98.2％；분별재불동반응온도하측정뇨전73.0、88.0、175.0、206.0、212.0 μg/L적5충뇨전표준물,상대오차범위위-2.8％(-5.9/212)～3.9％(6.9/175)；측정뇨전556.0μg/L화883.0μg/L적2충고뇨전표준물,상대오차범위위-0.7％(-7.0/883)～1.5％(8.1/556),측정결과균재급정치적불학정도범위내.결론 수정후적신방법비원표준방법대폭감소료폐액함신량,감소료배경오염병절성료시제.가직접취고전뇨양진행소화측정,피면료원표준방법측정고전뇨양수다배희석적희석오차화조작불편,간편역조작,병제고료측정정밀도화준학도.
Objective To introduce a newly revised method for determination of urinary iodine with low usage amount of arsenic trioxide and by As(Ⅲ)-Ce4+ spectrophotometry using ammonium persulfate digestion.Methods The newly revised method include:improved detection steps of 0.0-300.0 μ4g/L range urinary iodine,and increased detection steps of 300.0-1200.0 μg/L range urinary iodine,usage amount of arsenious acid solution was only a quarter of usage amount of the current standard method.The new modification for the national standard method was introduced and the method was evaluated on standard curve linearity and linear range,sample detection limit,precision and accuracy.Results The linear correlation coefficients d the 0.0-300 μg/L range and 300.0-1200.0 μg/L range calibration curve[C =a + b × lgA,C:iodine concentration,A:measuring absorbance] were -0.9995--1.0000,-0.9994--1.0000,respectively.The detection limit for iodine was 2.0 μg/L(0.25 ml of urine was tested).The relative standard deviations were 0.9％ (0.6/70.3)-3.3％(1.2/35.6) when measuring 12 urine samples with iodine conc entration of 35.6-265.5 μg/L,and 0.4％ (2.0/517.3)-2.2％ (7.2/330.1) when measuring 12 urine samples with iodine concentration of 330.0-1112.0 μg/L.The average recovery was 99.4％ with a range of 93.8％ (93.8/100)-103.9％(103.9/100) when measuring 15 urine samples with iodine concentration of 33.7-203.0 μg/L,and was 98.2％ with a range of 91.2％(501.8/550)-102.9％(411.7/400) when measuring 15 urine samples with iodine concentration of 330.0-783.0 μg/L.At different test temperature,the test results of five urinary iodine national standard materials with iodine concentration of 73.0,88.0,175.0,206.0,212.0 μg/L were all within the given value range and the relative deviation range was-2.8％(-5.9/212)-3.9％(6.9/175),and the test results of two urinary iodine national standard materials with iodine concentration of 556.0 and 883.0 μg/L were all within the given value range and the relative deviation range was-0.7％ (-7.0/883)-1.5％(8.1/556).Conclusions This newly modified method greatly reduces the amount of arsenic in liquid waste,reduces pollution,saving reagents,can directly access to urine samples with high iodine for digestion and determination,and this method is easier to be performed with better precision and accuracy,which is suitable to almost all routine laboratory test for measuring urinary iodine.